CN110048123A - Silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent and preparation method thereof - Google Patents
Silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent and preparation method thereof Download PDFInfo
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- CN110048123A CN110048123A CN201910355206.9A CN201910355206A CN110048123A CN 110048123 A CN110048123 A CN 110048123A CN 201910355206 A CN201910355206 A CN 201910355206A CN 110048123 A CN110048123 A CN 110048123A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent, the compound including few-wall carbon nanotube, graphene, dispersing agent and deionized water composition, the few-wall carbon nanotube fibrous structure, the graphene is laminated structure；The weight ratio of the few-wall carbon nanotube and graphene is 5~10:1；The weight ratio of the sum of weight of the few-wall carbon nanotube and graphene and dispersing agent is 4~8:1.Prepared by the present invention convenient, and product cost is low, and agglomeration is clearly better, and dispersion performance is significantly promoted.
Description
Technical field
The present invention relates to lithium ion battery preparation fields, and in particular to a kind of silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube
Waterborne conductive agent and preparation method thereof.
Background technique
Lithium ion secondary battery is a kind of novel high-energy secondary cell, with specific capacity is big, discharge voltage is high and steady, low
Warm nature can good, environmental-friendly, safety, the advantages that service life is long, self discharge is faint.The above-mentioned advantage of lithium ion secondary battery, causes
The attention and favor of countries in the world scientists, to promote the fast development of lithium ion secondary battery.Since the advent of the world, it is short
Between short recent two decades, it is a series of that lithium ion secondary battery has just been widely used in mobile phone, laptop, digital equipment etc.
In portable electronic product；Especially in recent years in the vehicles, aerospace, military affairs such as some key areas such as electric cars
The exploitation and application of the large-scale lithium ion secondary battery in equal fields are just unfolded in high gear.
The electrode reaction of lithium ion secondary battery includes the transmission of electronics and the transmission of ion, this requires that electrode will have
Good electric conductivity guarantees the unimpeded of electron propagation ducts；Necessary some pore structures, electrolyte of attracting deposit guarantee ion transmission
It is smooth.Only reach the requirement of these two aspects, just can guarantee that electrode active material has higher utilization rate and good circulation
Stability.The cathode of lithium ion secondary battery is frequently with graphite type material, such as: flake graphite, graphite microspheres and modified graphite
Microballoon etc..
These materials itself have preferable electric conductivity, and unnecessary addition conductive agent improves its electric conductivity in principle, but
It is that a small amount of conductive agent is added to improve contact resistance between negative electrode active material, keeps the electric conductivity at each position of electrode consistent；
Especially some fibre shape conductive agent can also improve the bonding stability of negative electrode material and increase the pore structure of electrode, in favor of
It attracts deposit electrolyte, improves the cyclical stability of electrode.
Graphite, acetylene black and carbon fiber it is conductive it is good, density is small, stable structure and chemical stability characteristic, often
It is used as the conductive agent of lithium ion secondary battery.If charge/discharge speed is slow, these conductive agents can play performance.But such as
Fruit is big multiplying power fast charging and discharging, can generate biggish polarization using the electrode of these conductive agents, lead to the utilization of active material
Rate decline.In order to improve the performance of lithium ion battery, the exploitation of novel conductive agent is extremely urgent.
Carbon nanotube is that one kind that is nested and being formed has " together graphene film seamless cylinder made of axis curling layer by layer
The tube-like materials of heart cylindrical structure ", diameter is in nanometer scale, and length is in micron dimension.Carbon nanotube crystallinity is high, while tube wall
There are the big pi bonds of delocalization, thus carbon nanotube has good conductive property.Carbon nanotube has fibrous structure, is conducive to
Effective conductive network and fixed electrode material are formed in electrode.In addition, specific surface area of carbon nanotube is big, there is porous structure,
It is easy to electrolyte of attracting deposit.Carbon nanotube conducting agent has apparent advantage compared with other conductive agents.
Minority enterprise is also in research and development conductive agent at present, but all there is price height, reunites than more serious, it is difficult to which dispersion etc. is asked
Topic.How reducing cost, solving the dispersion of carbon nanotube when in use is always industry focus of attention.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductives
Agent and preparation method thereof, it is convenient to prepare, and product cost is low, and agglomeration is clearly better, and dispersion performance is significantly promoted.
In order to solve the above-mentioned technical problems, the present invention provides a kind of silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube is aqueous
Conductive agent, the compound including few-wall carbon nanotube, graphene, dispersing agent and deionized water composition, the few-wall carbon nanotube
Fibrous structure, the graphene are laminated structure；
The weight ratio of the few-wall carbon nanotube and graphene is 5~10:1；
The weight ratio of the sum of weight of the few-wall carbon nanotube and graphene and dispersing agent is 4~8:1.
Further, the conductive agent is prepared for the cathode of lithium ion secondary battery, the material of cathode be flake graphite,
Modified natural graphite microballoon, artificial graphite microspheres, carbonaceous mesophase spherules, carbon fiber or nano-silicon.
Further, 3~100nm of caliber of the few-wall carbon nanotube, length are 0.6~200um.
Further, the dispersing agent is polyvinylpyrrolidone or polyvinyl alcohol.
Further, the total content of the few-wall carbon nanotube and graphene is 5.6~6.2%.
A kind of preparation method is used to prepare conductive agent described in above-mentioned any one, comprising the following steps:
Step 1) weighs few-wall carbon nanotube, graphene, dispersing agent and deionized water according to the proportion；
Few-wall carbon nanotube, graphene and dispersing agent, and high speed dispersion is added in step 2) in deionized water, and slurry is made
Material；
Or first dispersing agent is added in deionized water and stirs at low speed dispersion, it then adds graphene and stirs at low speed point
It dissipates, is eventually adding few-wall carbon nanotube, and high-speed stirred is dispersed, and slurry is made；
Slurry is milled into finely dispersed conductive agent by sand milling or colloid by step 3).
Further, high speed dispersion is using the vacuum stirring equipment for having cooling system.
Beneficial effects of the present invention:
1, application method is substantially identical with the application method of existing lithium ion secondary battery conductive agent, does not change existing lithium
The production line of ion secondary battery；The usage amount of conventional conductive agent is reduced simultaneously, while improving the overall performance of lithium battery；
2, graphene has the characteristics that purity is high, partial size is small, is evenly distributed, and large specific surface area, high surface and pine
Fill density it is low, although itself dispersibility it is not very ideal, with few-wall carbon nanotube it is compound after, the agglomeration of the two is bright
It is aobvious to improve, so that dispersion performance is significantly promoted.
3, the use of few-wall carbon nanotube advantageously forms effective conductive network, only has effective conductive mesh
Network could act on each other together with graphene, form a kind of synergistic effect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that conductive agent of the invention amplifies 20000 times；
Fig. 2 is the relation curve of negative discharge capacity and cycle-index in the case of three kinds of the present invention.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
What lithium ion battery negative material generallyd use is graphite carbon material, but its theoretical specific capacity only has 372mAh/
G, thus further increasing for lithium ion battery specific energy is limited, it is not able to satisfy increasingly developed high-energy Portable movable electricity
The demand in source, and that there are charge/discharge capacities is low for carbon material, high-rate charge-discharge capability is poor, and stability is poor etc. in the electrolyte
Problem.It is various existing for current carbon material in order to overcome the problems, such as, it is mainly studied at two aspects in the industry: on the one hand being passed through
Various physics and chemical means are modified carbon material, improve its chemical property, and on the other hand then concentrating on finding can be with
Substitute the new negative electrode material system of carbon material.
Nano silicon material with huge lithium storage content (theoretical capacity 4200mAh/g) due to being concerned.Silicon and lithium
Alloy can be formed: xLi+Si；Embedding personal structure is most common in Si/C composite negative pole material, and Si powder is dispersed in carbon
In the dispersible carriers such as pipe, graphite, two-phase or multiphase system of stable and uniform is formed.In charge and discharge process, Si is that electrochemistry is anti-
The transmission channel and structural support of ion, electronics are mainly played although carbon carrier also has removal lithium embedded performance in the activated centre answered
The effect of body.Si/C composite material not only can be reduced since nano-silicon to be dispersed in elastic and small bulk effect carbon parent
The volume change of electrode, reduce electrode surface solid electrolyte (Solid Electroly teInterphase, SEI) film due to
It is destroyed caused by volume change, and silicon is wrapped in carbon, can prevent the reunion of nano-silicon active body, to improve material
Cyclical stability.
New material is ineffective when using existing conductive agent, therefore the present invention provides a kind of universal conductive agent:
One embodiment of silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent of the invention, including few wall carbon are received
The compound that mitron (also referred to as carbon pipe), graphene, dispersing agent and deionized water form, few-wall carbon nanotube fibrous structure,
Graphene is laminated structure；Specifically, 3~100nm of caliber of few-wall carbon nanotube, length is 0.6~200um, generally, pipe
Diameter is bigger, and the length of few-wall carbon nanotube is shorter.It is found by numerous tests, the few-wall carbon nanotube of 10~50nm of caliber is used
It is best to make effect when conductive agent, because of its caliber, moderate length, relative to caliber for bigger few-wall carbon nanotube, pipe number
Mesh is more, and for, the longer carbon nanotube of length smaller relative to caliber, mutual winding is slighter, is easier to disperse,
So advantageously forming effective conductive network, only have effective conductive network, could make each other together with graphene
With forming a kind of synergistic effect.
Prepared by cathode of the conductive agent for lithium ion secondary battery, the main material of cathode is nano-silicon, naturally it is also possible to be
Flake graphite, modified natural graphite microballoon, artificial graphite microspheres, carbonaceous mesophase spherules, carbon fiber etc..And dispersing agent is poly- second
Alkene pyrrolidone (PVP) or polyvinyl alcohol (PVA).
Lithium-ion negative pole active material uses modified graphite microballoon HMSG2.8g, conductive agent 2.94g, binder
SBR0.14g, thickener CMC0.04g, is added in NMP, disperses 240~300 minutes in vacuum high speed disperser, viscosity control
System (is adjusted) in 4000~5000cp by the additional amount of NMP, and the discharging of 150 meshes, in 16 μm of thickness of aluminium foils, (specification is
60~80 μm of film on 350x0.016mm) are dried in 100 DEG C of vacuum drying ovens, and the electrode slice of φ 16 is made in punching；
Electrode slice is divided into 5 parts, is tested respectively:
Electrode slice one: using 16 μm of Cellgard2400 of thickness as diaphragm, LiPF6 solution is that electrolyte forms simulated battery,
The specific discharge capacity with 269mAh/g in 1.5C electric discharge is measured, 87% when 0.5C is reached.
Electrode slice two: using 16 μm of Cellgard2400 of thickness as diaphragm, LiPF6 solution is that electrolyte forms simulated battery,
The specific discharge capacity with 265mAh/g in 1.5C electric discharge is measured, 85% when 0.5C is reached.
Electrode slice three: using 16 μm of Cellgard2400 of thickness as diaphragm, LiPF6 solution is that electrolyte forms simulated battery,
The specific discharge capacity with 270mAh/g in 1.5C electric discharge is measured, 86% when 0.5C is reached.
Electrode slice four: using 16 μm of Cellgard2400 of thickness as diaphragm, LiPF6 solution is that electrolyte forms simulated battery,
The specific discharge capacity with 264mAh/g in 1.5C electric discharge is measured, 84% when 0.5C is reached.
Electrode slice five: using 16 μm of Cellgard2400 of thickness as diaphragm, LiPF6 solution is that electrolyte forms simulated battery,
The specific discharge capacity with 257mAh/g in 1.5C electric discharge is measured, 81% when 0.5C is reached.
Conductive agent is prepared using above-mentioned formula, by 4.69kg deionized water, polyvinylpyrrolidone (PVP) 60g is added, adds
Enter graphene 75g, add carbon nanotube (CNTs) 175g and ground after high-speed stirred mixes with sand mill or colloid mill
The slurry sample that system processing is 6.2% to get solid content.
Then adopt and prepare electrode slice in a like fashion, obtain electrode slice six, with 16 μm of Cellgard2400 of thickness be every
Film, LiPF6 solution are that electrolyte forms simulated battery, measure the specific discharge capacity with 243mAh/g in 1.5C electric discharge, reach
78% when to 0.5C.
It is compared in order to clearer, in the case where any conductive agent is not added, takes negative electrode active material
HMSG2.98g, binder SBR0.04g, thickener CMC0.14g.Electrode slice preparation, simulated battery assembling and test are the same as above-mentioned side
Formula is consistent.Electrode slice seven measures the specific discharge capacity with 102mAh/g in 1.5C electric discharge, reaches 33% when 0.5C.
It is above-mentioned high speed dispersion preparation when using the vacuum stirring equipment for having cooling system.
The chemical property table of composition and negative electrode material graphite HMSG composition electrode when prepared by conductive agent
The conductive agent of above-mentioned preparation is observed under scanning electron microscope, amplification factor is 20000 times, it can be seen that CNTs and stone
Black alkene is uniformly combined with each other, shown referring to Fig.1.
When combined conductive agent (Mix), one-component carbon nanotube (CNTs) is added or does not have to conductive agent (None) by electrode slice
Three kinds of situations, ion secondary battery cathode material lithium graphite (C) under 1.5C discharge-rate, discharge capacity and cycle-index
Relation curve is referring to shown in Fig. 2；The chart is bright to use aqueous combined conductive agent, and electric discharge of the electrode under the discharge-rate of 1.5C is held
Amount and cyclical stability are better than carbon nanotube and do not have to conductive agent.
In one embodiment, each component content are as follows: deionized water 4.69kg, polyvinylpyrrolidone (PVP) 34g, graphite
Alkene 46g, few-wall carbon nanotube (CNTs) 230g.
In one embodiment, each component content are as follows: deionized water 4.69kg, polyvinylpyrrolidone (PVP) 78g, graphite
Alkene 39g, few-wall carbon nanotube (CNTs) 193g.
In one embodiment, each component content are as follows: deionized water 4.69kg, polyvinylpyrrolidone (PVP) 34g, graphite
Alkene 92g, few-wall carbon nanotube (CNTs) 138.
In one embodiment, each component content are as follows: deionized water 4.69kg, polyvinylpyrrolidone (PVP) 78g, graphite
Alkene 78g, few-wall carbon nanotube (CNTs) 155g.
The application method of combined conductive agent of the invention is with other conductive agents, and slightly different, we develop compound
The additive amount of conductive agent will be according to the difference of battery material used and difference, the overall principle have been that the material of good conductivity can
With the additive amount of moderate reduction combined conductive agent, i.e. additive amount is inversely proportional with electric conductivity.The electric conductivity of negative electrode material is generally preferable,
The additive amount of combined conductive agent is generally 1~3%.Conductive agent additional amount is very few, and conductive network is not intensive enough；Conductive agent additional amount
Excessively, waste is not said, while increasing the dosage of binder, reduces the specific capacity of electrode.
Above embodiments are only to absolutely prove preferred embodiment that is of the invention and being lifted, and protection scope of the present invention is not
It is limited to this.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in guarantor of the invention
Within the scope of shield.Protection scope of the present invention is subject to claims.
Claims (7)
1. a kind of silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent, which is characterized in that including few-wall carbon nanotube,
The compound of graphene, dispersing agent and deionized water composition, the few-wall carbon nanotube fibrous structure, the graphene are piece
Shape structure；
The weight ratio of the few-wall carbon nanotube and graphene is 5~10:1；
The weight ratio of the sum of weight of the few-wall carbon nanotube and graphene and dispersing agent is 4~8:1.
2. silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent as described in claim 1, which is characterized in that described
Prepared by cathode of the conductive agent for lithium ion secondary battery, the material of cathode is flake graphite, modified natural graphite microballoon, artificial
Graphite microspheres, carbonaceous mesophase spherules, carbon fiber or nano-silicon.
3. silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent as described in claim 1, which is characterized in that described
3~100nm of caliber of few-wall carbon nanotube, length are 0.6~200um.
4. silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent as described in claim 1, which is characterized in that described
Dispersing agent is polyvinylpyrrolidone or polyvinyl alcohol.
5. silicon/carbon/graphite in lithium ion batteries alkene few-wall carbon nanotube waterborne conductive agent as described in claim 1, which is characterized in that described
The total content of few-wall carbon nanotube and graphene is 5.6~6.2%.
6. a kind of preparation method, which is characterized in that it is used to prepare conductive agent described in claim 1-5 any one, including with
Lower step:
Step 1) weighs few-wall carbon nanotube, graphene, dispersing agent and deionized water according to the proportion；
Few-wall carbon nanotube, graphene and dispersing agent, and high speed dispersion is added in step 2) in deionized water, and slurry is made；
Or first dispersing agent is added in deionized water and stirs at low speed dispersion, it then adds graphene and stirs at low speed dispersion,
It is eventually adding few-wall carbon nanotube, and high-speed stirred is dispersed, and slurry is made；
Slurry is milled into finely dispersed conductive agent by sand milling or colloid by step 3).
7. preparation method as claimed in claim 6, which is characterized in that high speed dispersion, which uses, has the vacuum stirring of cooling system to set
It is standby.
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Application publication date: 20190723 |